WO2009068219A1 - Calorimètre comportant un contenant de dissolution et une chemise d'eau - Google Patents

Calorimètre comportant un contenant de dissolution et une chemise d'eau Download PDF

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Publication number
WO2009068219A1
WO2009068219A1 PCT/EP2008/009818 EP2008009818W WO2009068219A1 WO 2009068219 A1 WO2009068219 A1 WO 2009068219A1 EP 2008009818 W EP2008009818 W EP 2008009818W WO 2009068219 A1 WO2009068219 A1 WO 2009068219A1
Authority
WO
WIPO (PCT)
Prior art keywords
pressure vessel
container
pressure
liquid
digestion
Prior art date
Application number
PCT/EP2008/009818
Other languages
German (de)
English (en)
Inventor
Hubert Pinhack
Original Assignee
Ika-Werke Gmbh & Co. Kg
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Ika-Werke Gmbh & Co. Kg filed Critical Ika-Werke Gmbh & Co. Kg
Priority to EP08853297A priority Critical patent/EP2212666B1/fr
Priority to US12/745,336 priority patent/US8356933B2/en
Priority to AT08853297T priority patent/ATE524715T1/de
Priority to BRPI0819843A priority patent/BRPI0819843B1/pt
Priority to CN2008801182584A priority patent/CN101878414B/zh
Priority to PL08853297T priority patent/PL2212666T3/pl
Priority to AU2008329146A priority patent/AU2008329146B2/en
Publication of WO2009068219A1 publication Critical patent/WO2009068219A1/fr
Priority to ZA2010/03181A priority patent/ZA201003181B/en
Priority to HK11100008.7A priority patent/HK1146114A1/xx

Links

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
    • G01K17/00—Measuring quantity of heat
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00—Investigating or analyzing materials by the use of thermal means
    • G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
    • G01N25/22—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on combustion or catalytic oxidation, e.g. of components of gas mixtures
    • G01N25/26—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on combustion or catalytic oxidation, e.g. of components of gas mixtures using combustion with oxygen under pressure, e.g. in bomb calorimeter

Definitions

  • the invention relates to a calorimeter with a digestion vessel containing a combustion chamber, in which a receiving device for a sample and an ignition device and at least one supply line for oxygen are provided with a surrounding the digestion vessel water jacket or liquid jacket, a projecting into the water or liquid jacket Temperature sensor and with an outer container comprising the water or liquid jacket.
  • Such calorimeters are in a variety of forms, for example from DE 43 14 454 C1 or DE 100 24 147 C1, known.
  • the digestion tank containing the combustion chamber must have a thick and stable jacket and, moreover, be made of high-quality material so that it does not disturb or influence the combustion and does not damage itself becomes.
  • the outer container is designed as a pressure vessel and the resulting pressure in a combustion in the drucknachbineden digestion vessel on the wall pressure over the water or liquid jacket, hereinafter called “water jacket” for simplicity, receives and that to compensate for thermal movements and pressure differences, the wall of the digestion container connected to its bottom via a dense pressure nachmetreden sliding seat or to the digestion container, a diaphragm, a bellows or a movable piston is arranged.
  • the invention enables the digestion vessel to be thin-walled in relation to the outer pressure vessel and its wall thickness to be less than the wall thickness of the pressure vessel.
  • An expedient embodiment of the invention can provide that the inside of the wall of the pressure vessel is provided with insulation for insulation against external influences and for reducing energy transport from the exclusion vessel via the surrounding incompressible liquid or the water to or into the pressure vessel , As a result, it is possible to warm up the liquid or the water, but not the pressure vessel, which could falsify the measurement.
  • the pressure vessel can thus absorb the pressure occurring during the combustion of a sample, it is itself heated only slightly and, together with the insulation located on its inside, keeps external influences away from the water jacket, so that touching distortions of the measurement result are at least largely avoided.
  • the insulation is an insulated container. This can be prefabricated in a simple and expedient manner and then inserted into the outer container.
  • An expedient embodiment, especially of the insulation can provide that this insulation or the insulating container is spaced from the inside of the pressure vessel or the inside of the pressure vessel only partially touched. As a result, an insulating space can still be kept free between the pressure vessel and the insulation, which improves the insulating effect.
  • At least the digestion container may consist of a temperature and / or chemical resistant material, for example of metal, ceramic and / or plastic. Even plastic is possible because the digestion tank itself can not absorb pressure, but transmits it via the water jacket to the outer pressure vessel.
  • the pressure vessel and / or the insulating container may be made of metal, ceramic and / or plastic. The choice of material can then be made according to which samples are usually burned and examined therein.
  • a further embodiment of the invention may provide that on the outside of the pressure vessel, an insulation or insulating sheath is arranged. This can serve to improve the switching-off of external influences. In addition, it can be avoided or saved an insulated container within the pressure vessel.
  • At least one means for moving the liquid or a stirrer may be provided in the space between decomposition vessel and pressure vessel filled by the incompressible liquid or the water in use. Thereby, the distribution of the heat occurring during the combustion of a sample can be accelerated.
  • a magnetic stirrer is provided or arranged in the space of the calorimeter filled in with use by the incompressible liquid or water.
  • the fluid circulation to be carried out in this space or intermediate space for rapid heat equalization can therefore take place with the magnetically drivable and movable part of a magnetic stirrer.
  • the circulation movement at the high pressures resulting from the combustion without a passage such as a wave or the like to the outside is possible.
  • the thermal development influencing the calorimetric process is avoided by sliding friction of such a shaft, which requires a seal which is effective against high pressure.
  • more than one temperature sensor may be provided in the intermediate space which is arranged between the decomposition container and the pressure vessel and which receives water or an incompressible liquid during use, wherein these several temperature sensors may preferably be evenly distributed. As a result, the measuring speed and the measuring accuracy can be increased.
  • one or more temperature sensors can be arranged on the outside of the pressure vessel. Thus, it can be checked whether and how much heat has possibly leaked through the pressure vessel or what temperature difference exists between the two sides of the wall of the pressure vessel.
  • a further embodiment of the invention can provide that a temperature control device for setting a constant temperature of this pressure vessel is provided on the pressure vessel. This can be achieved that external influences are turned off in the measurement.
  • the shape of the combustion chamber within the digestion container can be arbitrary and arched over at least a portion or be cylindrical over the entire height or designed as a bellows to allow a space-saving form, but not to pay attention to compressive strength, because the pressure is advantageously transmitted through the liquid jacket on the outer container serving as a pressure vessel.
  • the entire calorimeter can save space, so with a clear lower total volume than previous conventional calorimeters are produced. Its transport is correspondingly easy and simple, and correspondingly fast calorimetric measurements can be carried out at different points or places. In this case, because of the incompressibility of the liquid, even a low compressive yield or possibly a low extensibility of the digestion container may be sufficient.
  • Fig. 1 is a vertical section through a first embodiment of a calorimeter according to the invention.
  • Fig. 2 is a representation corresponding to FIG. 1 of a second embodiment of the calorimeter according to the invention.
  • Fig. 2 is a representation corresponding to FIG. 1 of a second embodiment of the calorimeter according to the invention.
  • a calorimeter designated as a whole by 1 serves to measure the heat of combustion of substances and for this purpose has a digestion vessel 3 containing a combustion chamber 2, in which a receiving device 4 for such a sample and an ignition device 5 as well as a supply line 6 for oxygen are provided.
  • the digestion tank 3 is in the usual way in a water bath, that is, it is surrounded by a water jacket 7, wherein instead of water, another incompressible liquid could be provided.
  • the supply line 7a to the water jacket 7 is provided in the bottom area.
  • a temperature sensor 8 protrudes into this water jacket 7 or liquid jacket in order to measure the heating occurring during the combustion of a sample. Furthermore, a water tank or liquid jacket 7 comprehensive outer container 9 is provided.
  • the outer container 9 is designed as a pressure vessel and takes the pressure arising at the wall 10 at a combustion in the decomposition vessel 3 through the liquid or water jacket 7, so that the wall 10 may have a relatively small thickness, which affects the heat transfer accordingly little.
  • the digestion vessel 3 is in relation to the external, designed as a pressure vessel
  • Deten outer container 9 is thin-walled, wherein the wall thickness of the digestion container 3 is significantly less than the wall thickness of the outer or pressure vessel 9, hereinafter also referred to as "pressure vessel 9" is.
  • the inside of the wall of the pressure vessel 9 is provided for isolation against external influences that could interfere with the measurement accuracy, and to reduce the energy transport from digestion vessel 3 via the surrounding water of the water jacket 7 in the pressure vessel 9 with an insulation which is an insulating container 11 in the exemplary embodiment, that therefore contains the water jacket 7.
  • an insulation which is an insulating container 11 in the exemplary embodiment, that therefore contains the water jacket 7.
  • an insulation or insulating sleeve 11 a is arranged on the outside of the pressure vessel 9, so that an insulating vessel 11 within the pressure vessel 9 can be dispensed with. It can be seen between this insulating sleeve 11a and the pressure vessel 9, an air gap 12a, which forms the outer insulation together with the insulating sleeve 11a. As a result, an energy transport from the pressure or outer container 9 to the environment can be reduced.
  • the decomposition container 3 but expediently also the pressure container 9 and optionally the insulating container 11 made of a temperature and / or chemical resistant material, for example of Me tall, ceramic and / or plastic, which saves weight.
  • the pressure container 9 and optionally the insulating container 11 made of a temperature and / or chemical resistant material, for example of Me tall, ceramic and / or plastic, which saves weight.
  • an insulation or insulation could be arranged on the outside of the pressure vessel 9, an insulation or insulation to avoid external influences even better.
  • a means for moving the liquid or water, namely a stirrer 13 is provided in the embodiment of FIG. 1, with which the water moves accordingly and thereby the prevailing or elevated temperature can be distributed quickly and evenly.
  • a means for moving the liquid or the water in this case a magnetic stirrer 13a, is provided in the space filled by the incompressible liquid or the water in use, ie in the water jacket 7, with which the liquid or the water also moves and thereby the prevailing or elevated temperature can be distributed quickly and evenly.
  • a means for moving the liquid or the water in this case a magnetic stirrer 13a
  • the magnetic stirrer 13 can be driven without contact in a known manner via a magnetic coupling.
  • the wall 10 of the digestion container 3 is connected to the bottom 14 via a sealed sliding seat 15.
  • the pressure compensation can also be done by a decomposition vessel arranged diaphragm, a bellows or a movable piston done.
  • a further temperature sensor 16 can be arranged on the outside of the pressure vessel 9, which is provided in the embodiment at the top.
  • a tempering device for setting a constant temperature of the pressure vessel 9 could be provided on the pressure vessel 9 in order to exclude external influences on the measurement result.
  • the calorimeter 1 has a digestion tank 3 with combustion chamber 2, in which a receiving device 4 for a sample and an ignition device 5 and at least one supply line 6 are provided for oxygen.
  • the digestion tank 3 is surrounded by a liquid or water jacket 7, in which at least one temperature sensor 8 protrudes.
  • the liquid or water jacket 7 is surrounded by an outer container 9, which is designed as a pressure vessel and receives the pressure resulting from the combustion of a sample in the digestion container 3 at the wall 10 due to the tight sliding seat 15 via the water or incompressible liquid.
  • the digestion tank 3 can be designed to be correspondingly thin-walled, so that the heat produced during the combustion of a sample passes correspondingly quickly to the temperature sensor (s) 8.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • General Physics & Mathematics (AREA)
  • Physics & Mathematics (AREA)
  • Biochemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analyzing Materials Using Thermal Means (AREA)
  • Devices For Use In Laboratory Experiments (AREA)
  • Packages (AREA)
  • Containers Having Bodies Formed In One Piece (AREA)

Abstract

L'invention concerne un calorimètre (1) présentant un contenant de dissolution (3) comportant une chambre de combustion (2) pourvue d'un dispositif de réception (4) pour un échantillon, un dispositif d'allumage (5) et au moins une conduite d'amenée d'oxygène (6). Le contenant de dissolution (3) est entouré par une chemise de liquide ou d'eau (7) dans laquelle au moins une sonde de température (8) fait saillie. La chemise de liquide ou d'eau (7) est entourée par un contenant extérieur (9) conçu en tant que contenant de pression, absorbant la pression produite lors de la combustion d'un échantillon dans le contenant de dissolution (3), sur la paroi (10) de celui-ci, en raison de l'ajustement serré (15) au-dessus de l'eau ou du liquide incompressible. Le contenant de dissolution (3) peut présenter des parois fines en conséquence, de telle manière que la chaleur produite lors de la combustion d'un échantillon est transmise rapidement à la ou aux sondes de température (8).
PCT/EP2008/009818 2007-11-29 2008-11-20 Calorimètre comportant un contenant de dissolution et une chemise d'eau WO2009068219A1 (fr)

Priority Applications (9)

Application Number Priority Date Filing Date Title
EP08853297A EP2212666B1 (fr) 2007-11-29 2008-11-20 Calorimètre comportant un contenant de dissolution et une chemise d'eau
US12/745,336 US8356933B2 (en) 2007-11-29 2008-11-20 Calorimeter with a digestion container and with a water jacket
AT08853297T ATE524715T1 (de) 2007-11-29 2008-11-20 Kalorimeter mit einem aufschlussbehälter und mit einem wassermantel
BRPI0819843A BRPI0819843B1 (pt) 2007-11-29 2008-11-20 calorímetro com recipiente de solubilização e com uma camisa de água.
CN2008801182584A CN101878414B (zh) 2007-11-29 2008-11-20 具有消解容器并具有水套的热量计
PL08853297T PL2212666T3 (pl) 2007-11-29 2008-11-20 Kalorymetr z naczyniem wewnętrznym i z płaszczem wodnym
AU2008329146A AU2008329146B2 (en) 2007-11-29 2008-11-20 Calorimeter with a digestion container and with a water jacket
ZA2010/03181A ZA201003181B (en) 2007-11-29 2010-05-05 Calorimeter with a degestion container and with a water jacket
HK11100008.7A HK1146114A1 (en) 2007-11-29 2011-01-03 Calorimeter with a digestion container and with a water jacket

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102007057463A DE102007057463B3 (de) 2007-11-29 2007-11-29 Kalorimeter mit einem Aufschlussbehälter und mit einem Wassermantel
DE102007057463.2 2007-11-29

Publications (1)

Publication Number Publication Date
WO2009068219A1 true WO2009068219A1 (fr) 2009-06-04

Family

ID=40351837

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2008/009818 WO2009068219A1 (fr) 2007-11-29 2008-11-20 Calorimètre comportant un contenant de dissolution et une chemise d'eau

Country Status (13)

Country Link
US (1) US8356933B2 (fr)
EP (1) EP2212666B1 (fr)
CN (1) CN101878414B (fr)
AT (1) ATE524715T1 (fr)
AU (1) AU2008329146B2 (fr)
BR (1) BRPI0819843B1 (fr)
DE (1) DE102007057463B3 (fr)
ES (1) ES2371137T3 (fr)
HK (1) HK1146114A1 (fr)
PL (1) PL2212666T3 (fr)
RU (1) RU2460979C2 (fr)
WO (1) WO2009068219A1 (fr)
ZA (1) ZA201003181B (fr)

Families Citing this family (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
ZA201003782B (en) * 2009-05-29 2011-02-23 John Anthony Bonnard Calorimeter
US20110164652A1 (en) * 2010-01-05 2011-07-07 Refalo Lee A Differential Thermoelectric Cooler Calorimeter
JP5908927B2 (ja) * 2011-03-11 2016-04-26 アライアンス フォー サステイナブル エナジー リミテッド ライアビリティ カンパニー エネルギー貯蔵システムとパワーエレクトロニクスを試験するための熱量計ならびにそれらの製造方法および使用方法
DE102011016956B3 (de) * 2011-04-13 2012-08-09 Ika-Werke Gmbh & Co. Kg Verfahren und Vorrichtung zum Kühlen eines Aufschlussbehälters eines Kalorimeters nach einer Benutzung
DE102011101733B4 (de) * 2011-05-17 2012-12-06 Ika-Werke Gmbh & Co. Kg Verbrennungskalorimeter mit einem Aufschlussgefäß
CN102519780A (zh) * 2011-10-29 2012-06-27 重庆川仪分析仪器有限公司 化学需氧量水质自动分析仪用消解装置
JP6076166B2 (ja) * 2013-03-26 2017-02-08 大陽日酸株式会社 燃焼・爆発試験装置
CN106018470B (zh) * 2016-05-19 2019-04-16 重庆大学 一种建筑墙体动态传热过程测试方法
DE102018104327B4 (de) * 2018-02-26 2021-11-04 Ika - Werke Gmbh & Co. Kg Kalorimeter
US11201358B1 (en) 2018-05-08 2021-12-14 United States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration Systems and methods for measuring a heat response of a battery cell in thermal runaway
CN113189139B (zh) * 2021-04-21 2022-06-14 武汉深维鼎测科技有限公司 基于壁温监测的氧弹装置

Citations (5)

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GB2089507A (en) * 1980-11-11 1982-06-23 Morat Kg Franz A Combustion Calorimeter
US4616938A (en) * 1983-01-10 1986-10-14 Leco Corporation Apparatus for measuring thermal and other quantities of substances
DE19542138C1 (de) * 1995-11-11 1996-10-10 Ika Analysentech Gmbh Verbrennungsbehälter für Kalorimeter
DE10024147C1 (de) * 2000-05-18 2001-10-04 Ika Werke Gmbh & Co Kg Verfahren und Vorrichtung zum Messen der Verbrennungswärme in einer Kalorimeterbombe
US20050008063A1 (en) * 2003-07-10 2005-01-13 Tiax Llc Low thermal inerta scanning adiabatic calorimeter

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US3718437A (en) * 1970-12-28 1973-02-27 P Paloniemi Isothermal calorimeter
SU1093913A1 (ru) * 1982-04-06 1984-05-23 Ленинградский Ордена Октябрьской Революции И Ордена Трудового Красного Знамени Технологический Институт Им.Ленсовета Адиабатический калориметр
DE3221548A1 (de) * 1982-06-08 1983-12-08 Milan Dr.rer.nat. 7808 Waldkirch Smisek Verbrennungs-kalorimeter
US4511263A (en) * 1983-07-12 1985-04-16 Prosen Edward J Bomb-type conduction calorimeter
DE4314454C1 (de) * 1993-05-03 1994-10-13 Ika Analysentech Gmbh Bombenkalorimeter
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Publication number Priority date Publication date Assignee Title
GB2089507A (en) * 1980-11-11 1982-06-23 Morat Kg Franz A Combustion Calorimeter
US4616938A (en) * 1983-01-10 1986-10-14 Leco Corporation Apparatus for measuring thermal and other quantities of substances
DE19542138C1 (de) * 1995-11-11 1996-10-10 Ika Analysentech Gmbh Verbrennungsbehälter für Kalorimeter
DE10024147C1 (de) * 2000-05-18 2001-10-04 Ika Werke Gmbh & Co Kg Verfahren und Vorrichtung zum Messen der Verbrennungswärme in einer Kalorimeterbombe
US20050008063A1 (en) * 2003-07-10 2005-01-13 Tiax Llc Low thermal inerta scanning adiabatic calorimeter

Also Published As

Publication number Publication date
RU2010119310A (ru) 2012-01-10
BRPI0819843B1 (pt) 2018-10-09
CN101878414B (zh) 2012-02-01
DE102007057463B3 (de) 2009-04-16
EP2212666A1 (fr) 2010-08-04
CN101878414A (zh) 2010-11-03
EP2212666B1 (fr) 2011-09-14
PL2212666T3 (pl) 2012-01-31
ES2371137T3 (es) 2011-12-27
HK1146114A1 (en) 2011-05-13
US8356933B2 (en) 2013-01-22
ATE524715T1 (de) 2011-09-15
ZA201003181B (en) 2011-01-26
RU2460979C2 (ru) 2012-09-10
BRPI0819843A2 (pt) 2015-06-16
AU2008329146B2 (en) 2014-04-24
US20100316087A1 (en) 2010-12-16
AU2008329146A1 (en) 2009-06-04

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